CN111411285A - Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy and preparation method thereof - Google Patents
Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Abstract
The invention discloses a high-strength and high-toughness medium-entropy alloy of Al and Ti microalloying and a preparation method thereof, wherein the alloy comprises the following components (CoNiFe)95Al5‑xTixWherein Co, Ni and Fe are in equal atomic ratio, and the value range of x is 1-4. The preparation process route of the alloy is as follows: vacuum arc melting, homogenizing annealing, forging (hot forging), homogenizing annealing, rolling (cold rolling), and annealing heat treatment. Firstly, proportioning Co, Ni, Fe, Al and Ti particles/blocks according to a certain proportion, smelting into ingots by adopting a vacuum arc melting method, and carrying out homogenization annealing; secondly, heating the cast ingot to a certain temperature, forging and forming, and then carrying out homogenizing annealing; and finally, rolling (cold rolling) the forged alloy to prepare a plate with the thickness of 1-1.5 mm, and carrying out annealing heat treatment at 600-1000 ℃. Rational plastic working and annealingThe heat treatment process can improve the obdurability of the alloy and prepare the medium-entropy alloy with excellent comprehensive performance.
Description
Technical Field
The invention relates to an Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy and a preparation method thereof, belonging to the technical field of material processing.
Background
The new alloy design concept provides that 5 or more than 5 elements are provided, and the alloy with 5 to 35 atomic percent of each element is high-entropy alloy, namely multi-principal-element alloy. In addition, high entropy alloys may also be defined in terms of entropy. Thermodynamically, entropy is a characterizationOne parameter of the degree of system clutter. The larger the degree of chaos, the larger the entropy of the system. Alloy materials can be divided into the following three major categories: low entropy alloys, i.e. conventional alloys, having one or two elements as the main constituent element (Δ S)mixLess than or equal to 0.69R); a medium entropy alloy comprising two to four main elements (0.69R. ltoreq. DELTA.S)mixLess than or equal to 1.61R); high entropy alloy comprising at least five main constituent elements (Δ S)mix≥1.61R)。
The medium-entropy alloy is between the traditional alloy (low-entropy alloy) and the high-entropy alloy, so that the outstanding performances of the high-entropy alloy, such as high strength and hardness, are maintained, the number of principal elements is reduced, the mixed entropy of the medium-entropy alloy is closer to that of the traditional alloy, and the medium-entropy alloy has better plastic processing performance.
At present, the preparation method of the entropy alloy in the block mainly comprises a vacuum arc melting method and a powder metallurgy method. The vacuum arc melting method can be used for melting the alloy with higher melting point, and can be used for melting more alloys at one time, so that volatile impurities and certain gases can be effectively removed. However, the cast alloy prepared by the method is easy to have the defects of large internal stress, component segregation, pores, shrinkage cavities and the like.
Due to the complex deformation mechanism, most of the related researches on the medium entropy alloy are focused on the casting state. At present, the subsequent processing technology of the as-cast medium entropy alloy mainly comprises two processes of forging and rolling. The defects of casting state looseness and the like can be eliminated by forging, and the microstructure is optimized, so that the mechanical property of the workpiece is generally superior to that of a casting made of the same material. The mechanical properties of the workpiece prepared by rolling are poor, the hardness is too high, and the mechanical properties can be recovered only by annealing.
The medium-entropy alloy has not received wide attention as a new alloy system, and relatively few reports of the influence of corresponding plastic deformation on the structure and the performance of the medium-entropy alloy exist. The method has the advantages that alloy components are reasonably designed, technological parameters of plastic deformation (forging and rolling) are optimized, the plastic deformation capacity of the medium-entropy alloy is continuously improved, and the method is an important direction for medium-entropy alloy research in the future. In order to improve the obdurability of the CoNiFe medium-entropy alloy, the medium-entropy alloy with better comprehensive performance is prepared by adding trace Al and Ti and performing plastic processing and annealing heat treatment at different temperatures.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a high-strength and high-toughness medium-entropy alloy formed by microalloying Al and Ti and a preparation method thereof, which are prepared by adopting a vacuum arc melting method (CoNiFe)95Al5-xTixThe (x is 1,2,3,4) medium entropy alloy, optimizes the technological parameters of forging, rolling and annealing heat treatment, improves the toughness of the alloy, and prepares the medium entropy alloy with excellent comprehensive performance.
The technical scheme is as follows: in order to achieve the aim, the Al and Ti microalloyed high-strength-toughness medium-entropy alloy comprises (CoNiFe)95Al5-xTixWherein Co, Ni and Fe are in equal atomic ratio, and the value range of x is 1-4.
The preparation method of the Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy comprises the following steps:
step 1, mixing Co, Ni, Fe, Al and Ti particles/blocks in proportion, placing the mixture into a vacuum arc furnace, and vacuumizing to 1 × 10-2～1×10-3Pa, the protective gas is argon, and the pressure in the furnace is 0.05-0.06 MPa; continuously overturning and remelting for at least 5 times in the smelting process, smelting into ingots, and carrying out homogenization annealing on the as-cast alloy ingots;
and 3, rolling the forged alloy block, and carrying out annealing heat treatment on the rolled alloy block.
Wherein the content of the first and second substances,
the purity of Co, Ni, Fe, Al and Ti grains/blocks in the step 1) is 99.97 wt.%, the smelting is vacuum arc smelting, and the value range of the smelting current is 100-300A.
And (2) carrying out homogenizing annealing at the temperature of 900-1100 ℃, keeping the temperature for 12-24 h, and cooling in a furnace.
And 2) heating the as-cast alloy ingot to 800-1000 ℃, placing the alloy ingot on a platform, forging the alloy ingot for multiple times by using a 20-40 kg forging machine, and finally forging the alloy ingot into a cuboid with the length, width and height of 60-70 mm, 20-30 mm and 3-5 mm respectively.
The temperature range of the homogenizing annealing in the step 2) is 900-1100 ℃, the heat preservation time is 1-12 h, and the cooling mode is air cooling.
And 3) rolling the forging block at room temperature according to the relative rolling reduction of 10%, 20%, 40%, 60%, 75%, 85% and 90% relative to the thickness of the original forging block, and finally obtaining the plate with the thickness of 1.0-1.5 mm.
And 3) annealing, wherein the temperature range is 600-1100 ℃, the heat preservation time is 1-12 h, and air cooling is carried out.
Has the advantages that: the invention has the following beneficial effects:
at room temperature, the CoNiFe intermediate entropy alloy has good plasticity, but poor strength and toughness. The invention adds trace Al and Ti with larger relative atomic radius, the total content is 5 percent, and the invention mainly enhances the solid solution strengthening effect. On the basis of ensuring that the matrix phase is a single-phase FCC structure, the precipitation of a strengthening phase is regulated and controlled through the change of the content of Al/Ti, so that the strength is improved and the good plasticity of the material is ensured. Meanwhile, different heat treatment processes are adopted to control the form and the quantity of precipitated phases.
The invention improves the structure and performance of the medium-entropy alloy through forging, rolling and proper heat treatment, improves the obdurability of the medium-entropy alloy and has better comprehensive performance.
Drawings
FIG. 1 is a photograph of (CoNiFe) prepared in example95Al4Ti1Hardness diagram of medium entropy alloy.
FIG. 2 shows the rolled state (CoNiFe) prepared in the example95Al3Ti2Stress-strain curves for the medium entropy alloys.
FIG. 3 shows the rolled state (CoNiFe) prepared in the example95Al2Ti3And (4) keeping the temperature of the medium-entropy alloy at 900 ℃ for 1h, and performing air cooling to obtain an EBSD (Electron Back-scattered diffraction) diagram.
FIG. 4 shows the annealing temperature of 1000 ℃ (CoNiFe) prepared in example95Al2Ti3And (3) a room-temperature tensile fracture morphology diagram of the medium-entropy alloy.
Detailed Description
The Al and Ti microalloyed high-strength-toughness medium-entropy alloy comprises (CoNiFe)95Al5- xTixWherein Co, Ni and Fe are in equal atomic ratio, and the value range of x is 1-4.
The preparation method comprises the following steps:
1) proportionally mixing Co, Ni, Fe, Al and Ti particles/blocks, putting them in vacuum arc furnace, vacuumizing to 1 × 10-2～1×10-3Pa, the protective gas is argon, and the pressure in the furnace is 0.05-0.06 MPa. And continuously overturning for at least 5 times in the smelting process, smelting into ingots, and carrying out homogenization annealing on the as-cast alloy ingots.
2) And forging the cast alloy ingot after the homogenization annealing, and carrying out homogenization annealing on the forged alloy block.
3) And heating the forged alloy block to 800-1000 ℃ for rolling, and carrying out annealing heat treatment on the rolled alloy block.
The purity of the Co, Ni, Fe, Al and Ti particles/chunks in step 1) were all 99.97 wt.%.
The smelting in the step 1) is vacuum arc smelting, and the value range of smelting current is 100-300A.
And (2) carrying out air cooling at the homogenization annealing temperature of 900-1100 ℃ for 12-24 h.
The forging process in the step 2) is that the as-cast alloy ingot is heated to 800-1000 ℃, placed on a platform, and forged for multiple times by adopting a 20-40 kg forging machine to finally forge the as-cast alloy ingot into a cuboid with the length, width and height of 60-70 mm, 20-30 mm and 3-5 mm respectively.
The temperature range of the homogenization annealing in the step 2) is 900-1100 ℃, the heat preservation time is 1-12 h, and the cooling mode is air cooling.
And 3) rolling the forging blocks subjected to homogenizing annealing at room temperature according to the relative reduction (relative to the thickness of the original forging blocks) of 10, 20, 40, 60, 75, 85 and 90% respectively, and finally obtaining the plate with the thickness of 1.0-1.5 mm.
The annealing temperature range in the step 3) is 600-1100 ℃, the heat preservation time is 1-12 h, and the cooling mode is air cooling.
Example 1
The Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy comprises the following components (CoNiFe)95Al4Ti1。
The preparation method of the Al and Ti microalloyed high-strength-toughness medium-entropy alloy comprises the following steps:
1) 16.52g of Co ingot, 16.45g of Ni ingot, 15.65g of Fe ingot, 0.96g of Al ingot and 0.42g of Ti ingot are put into a vacuum arc melting furnace and vacuumized to 1 × 10-3Pa, argon as protective gas, 0.05MPa of pressure in the furnace, and repeatedly turning and smelting for 5 times to obtain ingots. And carrying out homogenizing annealing on the as-cast alloy ingot at 1000 ℃, preserving heat for 12h, and cooling in air.
2) And forging the alloy ingot after the homogenizing annealing, and homogenizing annealing the forged alloy block.
Firstly, placing a forged alloy ingot in a muffle furnace to be heated to 900 ℃, then placing an as-cast alloy ingot on a platform, forging for multiple times by adopting a 40kg forging machine, and finally forging cuboids with the length, width and height of 60mm, 20mm and 4mm respectively. And then, the annealing temperature is 1000 ℃, the temperature is kept for 1h, and air cooling is carried out.
3) Rolling the forged alloy block, and carrying out annealing heat treatment on the rolled alloy block.
The homogenized and annealed forged blocks were rolled several times at room temperature according to relative reductions of 10%, 30%, 50%, 65%, and 75% (4 mm, each relative to the original height) to finally obtain a sheet of 1.0 mm. The annealing heat treatment temperature is 800 ℃, the heat preservation is carried out for 1h, and the medium entropy alloy is obtained after air cooling.
Example 2
The invention relates to an Al and Ti microalloyed high-toughness medium-entropy alloy (CoNiFe)95Al3Ti2。
The preparation method of the Al and Ti microalloyed high-strength-toughness medium-entropy alloy comprises the following steps:
1) 16.46g of Co ingot, 16.39g of Ni ingot, 15.60g of Fe ingot, 0.71g of Al ingot and 0.84g of Ti ingot are put into a vacuum arc melting furnace and vacuumized to 1 × 10-3Pa, protectionArgon is used as gas, the pressure in the furnace is 0.05MPa, and the process of turnover smelting is repeated for 5 times to smelt into ingots. And carrying out homogenizing annealing on the as-cast alloy ingot at 1000 ℃, preserving heat for 12h, and cooling in air.
2) And forging the alloy ingot after the homogenizing annealing, and homogenizing annealing the forged alloy block.
Firstly, placing a forged alloy ingot in a muffle furnace to be heated to 900 ℃, then placing an as-cast alloy ingot on a platform, forging for multiple times by adopting a 40kg forging machine, and finally forging cuboids with the length, width and height of 60mm, 20mm and 4mm respectively. And then, the annealing temperature is 1000 ℃, the temperature is kept for 1h, and air cooling is carried out.
3) Rolling the forged alloy block, and carrying out annealing heat treatment on the rolled alloy block.
The homogenized and annealed forged blocks were rolled several times at room temperature according to relative reductions of 10%, 30%, 50%, 65%, and 75% (4 mm, each relative to the original height) to finally obtain a sheet of 1.0 mm. The annealing heat treatment temperature is 800 ℃, the heat preservation is carried out for 1h, and the medium entropy alloy is obtained after air cooling.
Example 3
The invention relates to an Al and Ti microalloyed high-toughness medium-entropy alloy (CoNiFe)95Al2Ti3。
The preparation method of the Al and Ti microalloyed high-strength-toughness medium-entropy alloy comprises the following steps:
1) 16.40g of Co ingot, 16.33g of Ni ingot, 15.54g of Fe ingot, 0.47g of Al ingot and 1.26g of Ti ingot are put into a vacuum arc melting furnace and vacuumized to 1 × 10-3Pa, argon as protective gas, 0.05MPa of pressure in the furnace, and repeatedly turning and smelting for 5 times to obtain ingots. And carrying out homogenizing annealing on the as-cast alloy ingot at 1000 ℃, preserving heat for 12h, and cooling in air.
2) And forging the alloy ingot after the homogenizing annealing, and homogenizing annealing the forged alloy block.
Firstly, placing a forged alloy ingot in a muffle furnace to be heated to 900 ℃, then placing an as-cast alloy ingot on a platform, forging for multiple times by adopting a 40kg forging machine, and finally forging cuboids with the length, width and height of 60mm, 20mm and 4mm respectively. And then, the annealing temperature is 1000 ℃, the temperature is kept for 1h, and air cooling is carried out.
3) Rolling the forged alloy block, and carrying out annealing heat treatment on the rolled alloy block.
The homogenized and annealed forged blocks were rolled several times at room temperature according to relative reductions of 10%, 30%, 50%, 65%, and 75% (4 mm, each relative to the original height) to finally obtain a sheet of 1.0 mm. The annealing heat treatment temperature is 800 ℃, the heat preservation is carried out for 1h, and the medium entropy alloy is obtained after air cooling.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and any modifications or alterations that can be easily conceived by those skilled in the art are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A high-toughness medium-entropy Al-Ti microalloyed alloy features that its composition is (CoNiFe)95Al5- xTixWherein Co, Ni and Fe are in equal atomic ratio, and the value range of x is 1-4.
2. A method for preparing a high-toughness medium-entropy Al and Ti microalloyed alloy as defined in claim 1, wherein the method comprises the following steps:
step 1, mixing Co, Ni, Fe, Al and Ti particles/blocks in proportion, placing the mixture into a vacuum arc furnace, and vacuumizing to 1 × 10-2～1×10-3Pa, the protective gas is argon, and the pressure in the furnace is 0.05-0.06 MPa; continuously overturning and remelting for at least 5 times in the smelting process, smelting into ingots, and carrying out homogenization annealing on the as-cast alloy ingots;
step 2, forging the cast alloy ingot after the homogenization annealing, and carrying out homogenization annealing on the forged alloy block;
and 3, rolling the forged alloy block, and carrying out annealing heat treatment on the rolled alloy block.
3. The preparation method of the Al and Ti microalloyed high strength and toughness medium entropy alloy as claimed in claim 2, wherein the purity of Co, Ni, Fe, Al and Ti grains/blocks in the step 1) is 99.97 wt.%, the melting is vacuum arc melting, and the melting current value range is 100-300A.
4. The preparation method of the Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy as claimed in claim 2, characterized in that the homogenizing annealing in the step 1) is carried out at 900-1100 ℃ for 12-24 h, and the cooling mode is furnace cooling.
5. The preparation method of the Al and Ti microalloyed high strength and toughness medium entropy alloy as claimed in claim 2, wherein the forging process in the step 2) is that an as-cast alloy ingot is heated to 800-1000 ℃, placed on a platform, and forged for multiple times by a forging machine of 20-40 kg, and finally forged into a cuboid with the length, width and height of 60-70 mm, 20-30 mm and 3-5 mm respectively.
6. The preparation method of the Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy as claimed in claim 2, wherein the homogenizing annealing temperature in the step 2) is 900-1100 ℃, the heat preservation time is 1-12 h, and the cooling mode is air cooling.
7. The preparation method of the Al and Ti microalloyed high strength and toughness medium entropy alloy as claimed in claim 2, wherein the rolling process in the step 3) is to roll the forging block at room temperature according to the relative reduction of 10%, 20%, 40%, 60%, 75%, 85% and 90% relative to the thickness of the original forging block, and finally obtain a plate with the thickness of 1.0-1.5 mm.
8. The method for preparing the Al and Ti microalloyed high-strength and toughness medium-entropy alloy as claimed in claim 2, wherein the annealing in the step 3) is carried out at the temperature of 600-1100 ℃ for 1-12 h, and air cooling is carried out.
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Cited By (12)
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| CN111876646A (en) * | 2020-07-31 | 2020-11-03 | 东北大学 | Preparation method of high-strength-ductility medium-entropy alloy strip |
| CN112813332A (en) * | 2021-01-07 | 2021-05-18 | 青海大学 | High-entropy alloy based on solid solution and precipitation strengthening effect and preparation method thereof |
| CN112877619A (en) * | 2021-01-12 | 2021-06-01 | 中北大学 | High tensile strength (CoCrNi) Al3Ti3Preparation method of medium-entropy alloy |
| CN112893468A (en) * | 2021-02-08 | 2021-06-04 | 太原理工大学 | Method for improving strength of Fe-Mn-Cr-Ni high-entropy alloy through corrugated rolling and plain rolling process |
| CN113430445A (en) * | 2021-06-21 | 2021-09-24 | 哈尔滨工程大学 | FeCrNiAlMoNb high-entropy alloy and preparation method thereof |
| CN113528921A (en) * | 2021-06-23 | 2021-10-22 | 沈阳航空航天大学 | C-containing high-performance multi-principal-element high-entropy alloy and preparation method thereof |
| CN113652591A (en) * | 2021-07-22 | 2021-11-16 | 中国科学院金属研究所 | Ti-rich high-entropy alloy with high specific strength, high plasticity and high toughness and preparation thereof |
| CN114457270A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | L12Medium-entropy alloy with particles strongly plasticized and preparation method thereof |
| CN115233075A (en) * | 2022-07-29 | 2022-10-25 | 大连理工大学 | Ultrahigh-strength-toughness high-entropy alloy, and preparation method and application thereof |
| CN115354202A (en) * | 2022-07-05 | 2022-11-18 | 西北工业大学 | High-toughness material suitable for differential backfill spot welding tool and preparation method |
| CN115505812A (en) * | 2022-09-16 | 2022-12-23 | 华东理工大学 | Soft magnetic medium-entropy alloy and preparation method and application thereof |
| CN115537627A (en) * | 2022-09-19 | 2022-12-30 | 华东理工大学 | Anti-fatigue medium-entropy alloy and preparation method thereof |
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| CN112813332A (en) * | 2021-01-07 | 2021-05-18 | 青海大学 | High-entropy alloy based on solid solution and precipitation strengthening effect and preparation method thereof |
| CN112877619A (en) * | 2021-01-12 | 2021-06-01 | 中北大学 | High tensile strength (CoCrNi) Al3Ti3Preparation method of medium-entropy alloy |
| CN112893468A (en) * | 2021-02-08 | 2021-06-04 | 太原理工大学 | Method for improving strength of Fe-Mn-Cr-Ni high-entropy alloy through corrugated rolling and plain rolling process |
| CN113430445A (en) * | 2021-06-21 | 2021-09-24 | 哈尔滨工程大学 | FeCrNiAlMoNb high-entropy alloy and preparation method thereof |
| CN113528921A (en) * | 2021-06-23 | 2021-10-22 | 沈阳航空航天大学 | C-containing high-performance multi-principal-element high-entropy alloy and preparation method thereof |
| CN113652591A (en) * | 2021-07-22 | 2021-11-16 | 中国科学院金属研究所 | Ti-rich high-entropy alloy with high specific strength, high plasticity and high toughness and preparation thereof |
| CN114457270A (en) * | 2021-12-31 | 2022-05-10 | 西安理工大学 | L12Medium-entropy alloy with particles strongly plasticized and preparation method thereof |
| CN114457270B (en) * | 2021-12-31 | 2023-01-31 | 西安理工大学 | L1 2 Medium-entropy alloy with strong particle plasticization and preparation method thereof |
| CN115354202A (en) * | 2022-07-05 | 2022-11-18 | 西北工业大学 | High-toughness material suitable for differential backfill spot welding tool and preparation method |
| CN115233075A (en) * | 2022-07-29 | 2022-10-25 | 大连理工大学 | Ultrahigh-strength-toughness high-entropy alloy, and preparation method and application thereof |
| CN115233075B (en) * | 2022-07-29 | 2023-02-14 | 大连理工大学 | Ultrahigh-strength-toughness high-entropy alloy, and preparation method and application thereof |
| CN115505812A (en) * | 2022-09-16 | 2022-12-23 | 华东理工大学 | Soft magnetic medium-entropy alloy and preparation method and application thereof |
| CN115537627A (en) * | 2022-09-19 | 2022-12-30 | 华东理工大学 | Anti-fatigue medium-entropy alloy and preparation method thereof |
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